CN108530338A - A method of extending the refined tryptophan of equipment life - Google Patents
A method of extending the refined tryptophan of equipment life Download PDFInfo
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- CN108530338A CN108530338A CN201810412901.XA CN201810412901A CN108530338A CN 108530338 A CN108530338 A CN 108530338A CN 201810412901 A CN201810412901 A CN 201810412901A CN 108530338 A CN108530338 A CN 108530338A
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- tryptophan
- refined
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- equipment life
- membrane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of method of refined tryptophan more particularly to a kind of methods for the refined tryptophan extending equipment life, belong to chemical technology field.The present invention is by the method for nanofiltration membrane one one-step refining tryptophan of progress compared with current refining technique, and the channel of nanofiltration membrane is wider and material acid-alkali-corrosive-resisting, nanofiltration membrane both ends of the surface carry out end face coating using ceramic coating, and advantage is：Fouling membrane can not only be alleviated, but also filtering accuracy is high, service life is long, is expected to the long life as a kind of refined tryptophan and Simple process.
Description
Technical field
The present invention relates to the method for refined tryptophan a kind of more particularly to a kind of refined tryptophans extending equipment life
Method belongs to chemical technology field.
Background technology
L-Trp is human body and the necessary amino acid that animal itself can not synthesize, and is widely used in food, feed adds
Add the industries such as agent and medicine.According to measuring and calculating, the demand in world L-Trp market is more than 1,000,000 tons/year, and the world in 2010
Tryptophan production capacity is 1.47 ten thousand tons/year, therefore has preferable market prospects.Currently, tryptophan extraction is divided into two steps,
That is crude product extraction and fine work extraction.Crude product is extracted, in the industrial production, the general method for using 50 nm microfiltration of ceramic membrane,
Remove big molecular impurity.Fine work is extracted, the general multistep processes removal being combined using organic material NF membrane and activated carbon
Small molecular weight impurity.However, tryptophan system includes the impurity such as a large amount of albumen, pigment and inorganic salts.For organic nanofiltration membrane work
Skill, fouling membrane are serious.In production, it is both needed to carry out long-time cleaning to film surface using strong oxidizer or highly basic daily.According to
Manufacturer feeds back, and organic nanofiltration membrane technique changes the film period at 6 months to 1 year, and later maintenance cost greatly improves.It is prior
It is that, since organic nanofiltration membrane fouling membrane is serious, refining effect is affected, need to be further taken off in conjunction with activated carbon process
Color, and activated carbon process service life only 1-3 months, such as CN101863822B- colors in one one-step refining method extraction zymotic fluid
A kind of new process of the separation and Extraction L-Trp from zymotic fluid of patent and CN101812009A- of the production method of propylhomoserin it is special
It in profit, is required to be decolourized with activated carbon, and time to decoloration and temperature require.Therefore, existing refined color ammonia
Sour technique has that process section complexity and service life are short.
Invention content
The purpose of the present invention is for the prior art, there are the short defect of process section complexity and service life of equipment, propositions one
The method that kind extends the refined tryptophan of equipment life improves technique service life.
The present invention solves technical problem by the following technical programs：A kind of side for the refined tryptophan extending equipment life
Method includes the following steps：
Step 1: concentrated broth --- nanofiltration membrane filtration will be packed into through the pretreated L-Trp crude product of 50nm ceramic membranes
10 times of concentration is carried out in the material liquid tank of device, respectively obtains tryptophan concentrate and tryptophan penetrating fluid；
Step 2: preparing finished product --- the water for accounting for total processing volume 20% -40% is packed into the material liquid tank of the concentrate containing tryptophan
In, it dialyses by nanofiltration membrane, obtains tryptophan penetrating fluid, the tryptophan that the tryptophan penetrating fluid and the first step are obtained
Penetrating fluid is mixed to get mixed liquor, and the mixed liquor obtains L-Trp finished product through evaporative crystallization;
Step 3: cleaning ceramic NF membrane --- after the completion of step 2, with 1% -3%NaOH or NaClO cleaning agents of membrane, carry out film
Cleaning.
The thickening temperature of step 1 described in the above method is 30 DEG C -60 DEG C, and crossflow velocity is 3 m/s -5 m/s.
The dialysis temperature of the step 2 is 20 DEG C -50 DEG C and crossflow velocity is 2 m/s -5 m/s.Evaporative crystallization
Step is the evaporator that mixed liquor enters 70-85 DEG C, has been concentrated into when a large amount of crystal are precipitated and has stopped, concentrate is squeezed into crystallizing tank
It is cooled to 5-15 DEG C, crystallization time 6-8h obtains L-Trp finished product.
The Membrane cleaning time of the step 3 is 2-3 hours.
The nanofiltration membrane material is TiO2Or ZrO2Or Ti/Zr is compound, molecular cut off is 500 Da-5000
Da。
The nanofiltration membrane both ends of the surface of the step 1 and step 2 use TiO2Or ZrO2Or Ti/Zr composite coatings carry out
End face is applied coated with ceramic membrane equipment sealing effect is ensured, the operating pressure of nanofiltration membrane is 1-2MPa.
The above method carries out the repetitive process for concentrating and dialysing again after Membrane cleaning.
The present invention is compared with current process for refining, and the channel of nanofiltration membrane is wider and material acid-alkali-corrosive-resisting, ceramics are received
Filter membrane both ends of the surface carry out end face using ceramic coating and apply coated with guarantee ceramic membrane equipment sealing effect, and advantage is：Not only
Fouling membrane can be alleviated, and filtering accuracy is high, service life is long, be expected to as a kind of refined tryptophan long life and
Simple process.
Description of the drawings
Fig. 1 is TiO in one embodiment of the invention2Nanofiltration membrane refines the variations of flux figure of tryptophan.
Fig. 2 is ZrO in another embodiment of the present invention2Nanofiltration membrane refines the variations of flux figure of tryptophan.
Fig. 3 is the variations of flux figure that Ti/Zr nanofiltration membranes refine tryptophan in further embodiment of the present invention.
Fig. 4 is the process flow diagram of the present invention.
Specific implementation mode
Embodiment one
The material liquid tank of ceramic membrane filter device will be packed by the zymotic fluid of the pretreated crude product containing L-Trp of 50nm ceramic membranes
In.In sealed environment, temperature is 40 DEG C -50 DEG C, under conditions of pressure is 1 Mpa and crossflow velocity is 5 m/s, through 3000
DaTiO2After nanofiltration membrane concentrates 10 times, respectively obtains containing pigment, albumen and remain the concentrate of tryptophan and remove impurity
Tryptophan penetrating fluid.In sealed environment, temperature is 30 DEG C -40 DEG C, the item that pressure is 1 Mpa and crossflow velocity is 5 m/s
Under part, total processing 20% water of volume will be accounted for and be added in the material liquid tank equipped with concentrate, after nanofiltration membrane is dialysed, be removed
The tryptophan penetrating fluid of impurity.As seen from Figure 1, the average flux of the above process is 39 L/ (m2 h).By above-mentioned tryptophan
It after penetrating fluid mixing, into 85 DEG C of evaporator, has been concentrated into when a large amount of crystal are precipitated and has stopped, concentrate is squeezed into crystallizing tank drop
For temperature to 15 DEG C, crystallization time 8h obtains L-Trp finished product.On the other hand, concentrate is emptied, then will contains 1%NaOH's
Water is fitted into the material liquid tank of ceramic membrane filter device, and cleaning 3 hours is carried out to film.Finally, the purity of prepared finished product is 99.6
%, ash content are 0.36 %, and specific rotatory power is -30.4 °, and yield is 98 %, reaches finished product index.Its process lifetime is 5 years.
Embodiment two
The feed liquid of ceramic membrane filter device will be packed by the pretreated zymotic fluid containing L-Trp crude product of 50nm ceramic membranes
In tank.In sealed environment, temperature is 50-60 DEG C, and pressure is 1.5 MPa, under conditions of crossflow velocity is 3 m/s, through 5000 Da
ZrO2After nanofiltration membrane is concentrated to 10 times, respectively obtains containing pigment, albumen and remain the concentrate of tryptophan and remove impurity elimination
The tryptophan penetrating fluid of matter.It it is 40-50 DEG C in temperature in sealed environment, pressure is 1.5 MPa, and crossflow velocity is the item of 2 m/s
Under part, total processing 40 % water of volume will be accounted for and be added in the material liquid tank equipped with concentrate, after nanofiltration membrane is dialysed, be removed
The tryptophan penetrating fluid of impurity.As seen from Figure 2, the average flux of the above process is 38 L/ (m2 h).By above-mentioned tryptophan
It after penetrating fluid mixing, into 70 DEG C of evaporator, has been concentrated into when a large amount of crystal are precipitated and has stopped, concentrate is squeezed into crystallizing tank drop
For temperature to 5 DEG C, 6 h of crystallization time obtains L-Trp finished product.On the other hand, concentrate is emptied, then will contains 3 %NaClO
Water be fitted into the material liquid tank of ceramic membrane filter device, to film carry out cleaning 2 hours.Finally, the purity of prepared finished product is
99.6 %, ash content are 0.36 %, and specific rotatory power is -30.4 °, and yield is 98 %, reaches finished product index.Its process lifetime is
8 years.
Embodiment three
It will be by the pretreated material liquid tank for being packed into ceramic membrane filter device containing L-Trp crude product zymotic fluid of 50nm ceramic membranes
In.In sealed environment, temperature is 50-60 DEG C, and pressure is 2 MPa, under conditions of crossflow velocity is 4 m/s, the Ti/ through 500 Da
After Zr nanofiltration membranes are concentrated to 10 times, the color containing pigment, the concentrate of protein residue tryptophan and removing impurity is respectively obtained
Propylhomoserin penetrating fluid.In sealed environment, temperature is 20-30 DEG C, and pressure is 1.5 MPa, will under conditions of crossflow velocity is 3 m/s
It accounts for total processing 30 % water of volume to be added in the material liquid tank equipped with concentrate, after nanofiltration membrane is dialysed, be removed impurity
Tryptophan penetrating fluid.The average flux of the above process is 40 L/ (m it can be seen from figure 3 above2 h).Above-mentioned tryptophan is permeated
It after liquid mixing, into 80 DEG C of evaporator, has been concentrated into when a large amount of crystal are precipitated and has stopped, concentrate is squeezed into crystallizing tank cooling
To 10 DEG C, 7 h of crystallization time obtains L-Trp finished product.On the other hand, concentrate is emptied, then will contains 2%NaOH's
Water is fitted into the material liquid tank of ceramic membrane filter device, to 2.5 h of Membrane cleaning.Finally, the purity of prepared finished product is 99.6 %, ash
It is divided into 0.40%, specific rotatory power is -30.6 °, and yield is 97 %.Its process lifetime is 6 years.
Fig. 4 is the process flow diagram of above-described embodiment, it is seen that its processing step is simple.Tryptophan in above-described embodiment
Product quality reaches Chinese Pharmacopoeia standard, and the service life is substantially better than the prior art service life.
In addition to above-mentioned implementation, the present invention can also have other embodiment.It is all to be formed using equivalent substitution or equivalent transformation
Technical solution, fall within the scope of protection required by the present invention.
Claims (7)
1. a kind of method for the refined tryptophan extending equipment life, includes the following steps：
Step 1: concentrated broth --- the pretreated L-Trp crude product of 50nm ceramic membranes will be passed through and be packed into nanofiltration membrane mistake
It filters and carries out 10 times of concentration in the material liquid tank of device, respectively obtain tryptophan concentrate and tryptophan penetrating fluid；
Step 2: preparing finished product --- the water for accounting for total processing volume 20% -40% is packed into the material liquid tank of the concentrate containing tryptophan
In, it dialyses by nanofiltration membrane, obtains tryptophan penetrating fluid, the tryptophan that the tryptophan penetrating fluid and the first step are obtained
Penetrating fluid is mixed to get mixed liquor, and the mixed liquor obtains L-Trp finished product through evaporative crystallization;
Step 3: cleaning ceramic NF membrane --- after the completion of step 2, with 1% -3%NaOH or NaClO cleaning agents of membrane, carry out film
Cleaning.
2. extending the method for the refined tryptophan of equipment life according to claim 1, it is characterised in that：The step 1
Thickening temperature is 30 DEG C -60 DEG C, and crossflow velocity is 3 m/s -5 m/s.
3. extending the method for the refined tryptophan of equipment life according to claim 1, it is characterised in that：The step 2
Dialysis temperature is 20 DEG C -50 DEG C and crossflow velocity is 2 m/s -5 m/s.
4. extending the method for the refined tryptophan of equipment life according to claim 3, it is characterised in that：The step of evaporative crystallization
Suddenly it is the evaporator that mixed liquor enters 70~85 DEG C, has been concentrated into when a large amount of crystal are precipitated and has stopped, concentrate is squeezed into crystallization
Tank is cooled to 5~15 DEG C, and 6~8h of crystallization time obtains L-Trp finished product.
5. extending the method for the refined tryptophan of equipment life according to claim 1, it is characterised in that：The step 3
The Membrane cleaning time is 2-3 hours.
6. extending the method for the refined tryptophan of equipment life according to claim 1, it is characterised in that：The nanofiltration
Membrane material is TiO2Or ZrO2Or Ti/Zr is compound, molecular cut off is 500 Da-5000 Da.
7. extending the method for the refined tryptophan of equipment life according to claim 1, it is characterised in that：The step 1 and
The nanofiltration membrane both ends of the surface of step 2 use TiO2Or ZrO2Or Ti/Zr composite coatings carry out end face coating, nanofiltration membrane
Operating pressure is 1-2MPa.
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| CN201810412901.XA CN108530338A (en) | 2018-05-03 | 2018-05-03 | A method of extending the refined tryptophan of equipment life |
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| CN201810412901.XA CN108530338A (en) | 2018-05-03 | 2018-05-03 | A method of extending the refined tryptophan of equipment life |
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| CN108530338A true CN108530338A (en) | 2018-09-14 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060172058A1 (en) * | 2004-02-18 | 2006-08-03 | Dominion Nutrition, Inc. | Concentrated-protein food product and process |
| CN101863822A (en) * | 2010-06-17 | 2010-10-20 | 河南巨龙淀粉实业有限公司 | Production method for extracting tryptophan from fermentation liquor by one-step refining |
| CN102703535A (en) * | 2012-06-19 | 2012-10-03 | 江苏久吾高科技股份有限公司 | New technology for producing acrylamide by using ceramic membrane bioreactor |
| CN103360080A (en) * | 2013-07-18 | 2013-10-23 | 南京工业大学 | Improved method for preparing ceramic nanofiltration membrane by sol-gel method |
| CN105384714A (en) * | 2015-12-18 | 2016-03-09 | 南京工业大学 | Decolorizing and refining process of sodium dehydroacetate |
-
2018
- 2018-05-03 CN CN201810412901.XA patent/CN108530338A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060172058A1 (en) * | 2004-02-18 | 2006-08-03 | Dominion Nutrition, Inc. | Concentrated-protein food product and process |
| CN101863822A (en) * | 2010-06-17 | 2010-10-20 | 河南巨龙淀粉实业有限公司 | Production method for extracting tryptophan from fermentation liquor by one-step refining |
| CN102703535A (en) * | 2012-06-19 | 2012-10-03 | 江苏久吾高科技股份有限公司 | New technology for producing acrylamide by using ceramic membrane bioreactor |
| CN103360080A (en) * | 2013-07-18 | 2013-10-23 | 南京工业大学 | Improved method for preparing ceramic nanofiltration membrane by sol-gel method |
| CN105384714A (en) * | 2015-12-18 | 2016-03-09 | 南京工业大学 | Decolorizing and refining process of sodium dehydroacetate |
Non-Patent Citations (1)
| Title |
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| 范益群等: ""陶瓷纳滤膜制备与应用研究进展"", 《化工进展》 * |
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